| Summary: | Per- and polyfluoroalkyl substances (PFASs) are increasingly recognized as emerging contaminants, with some classified as persistent organic pollutants (POPs) and four recently regulated in food in the EU. However, due to the large structural diversity of PFASs, comprehensive monitoring remains essential. This study aimed to develop and apply a suspect and non-targeted screening approach to identify PFASs beyond those conventionally monitored in foodstuffs. The methodology combined optimized QuEChERS sample preparation, LC-HRMS acquisition, and prioritization of fluorinated signals, applying both suspect screening (SS) and non-targeted screening (NTS) strategies. Compared to targeted solid-phase extraction (SPE) coupled with MS/MS (QqQ) acquisition, this approach detected a broader range of PFASs in various food samples. Notably, as one of the first studies to apply NTS—a method typically used in environmental analysis—to food, it demonstrated the ability to detect both known and previously unlisted PFASs, such as PFPrA in an egg sample. This expanded approach enhances exposure assessment and supports the implementation of HRMS-based strategies for regulatory control and risk assessment.
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